CN102626116A - Plant pesticide and its preparation method - Google Patents
Plant pesticide and its preparation method Download PDFInfo
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- CN102626116A CN102626116A CN2011101713002A CN201110171300A CN102626116A CN 102626116 A CN102626116 A CN 102626116A CN 2011101713002 A CN2011101713002 A CN 2011101713002A CN 201110171300 A CN201110171300 A CN 201110171300A CN 102626116 A CN102626116 A CN 102626116A
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Abstract
The invention discloses a plant pesticide and its preparation method. The plant pesticide comprises the following components of: by weight, 1-30% of eucalyptole mother liquor, 5-20% of an emulsifier and the balance being anhydrous ethanol. The preparation method comprises the following steps of: preparing of the eucalyptole mother liquor and mixing. Based on a lot of indoor screening, traditional Chinese herbal medicines such as rhizoma atractylodis and the like are used as the main raw materials according to the proportion of Eucalyptus globulus to extract and process mother liquor, followed by the addition of auxiliary agents such as the emulsifier, anhydrous ethanol and the like. The plant pesticide provided by the invention is the first design at home and abroad; and reagents used have little toxicity and are environmentally friendly and safe when in use.
Description
Technical field
The present invention relates to a kind of insecticide, relate in particular to vegetative insecticide and preparation method thereof.
Background technology
Though chemical synthetic pesticide is still the important means of control diseases and pests of agronomic crop because of its control efficiency is good, speed is fast at present, application quantity is very big; But because abuse or itself problem unreasonably; Produced serious negative effect, promptly so-called " 3R " problem: residue of pesticide (Residue) cause environmental pollution, the infringement human and livestock health; The serious disease incidences of disease such as people's cancer, cardiovascular disease, hepatopathy heighten now, and this has some relations with environmental pollution; Chemical pesticide also is prone to develop immunity to drugs (Resistance), thereby makes damage by disease and insect be difficult to control; Chemical synthetic pesticide is big to natural enemy lethality, destroys the ecological balance, causes damage by disease and insect rampant (Resurgence) more easily.Research to the botanical pesticide active substance both at home and abroad has two purposes.The one, from plant, seek the lead compound of synthetic new chemical pesticide, the most successful example is like the lead compound of the pyrethrin pesticide that comes from Dalmatian chrysanthemum, comes from the lead compound etc. of the imidacloprid pesticide of nicotine.The 2nd, directly use plant resource explorations new plant agricultural chemicals with pesticidal active substance.Be main then because of resource shortage mostly abroad with first purpose.China is because of vast territory and abundant resources, and plant resources is abundant, and a lot of plants have cultivation history.Therefore, mostly direct appliable plant resource, exploitation botanical pesticide.The domestic plant pesticide of having developed is many with the matrine preparation mainly at present.Other also has chinaberry element, nicotine, Wormseed element, jervine, Celastrus angulatus, rotenone etc.These botanical pesticides are that the production of crops non-polluted cultivation and green food plays a good role.But for various reasons, the existing plant pesticide kind of China is dull, and the active compound of declaring is in the majority with matrine.Other kind belongs to new monoids such as alkaloids, terpenes, lactone mostly and relates to less.This situation might cause certain resource, and supply falls short of demand, causes starving, influences the production development of these botanical pesticides.Therefore in the botanical pesticide industry, press for the research and development new varieties, new active compound.New through looking into, domestic and international blue gum of no use and rhizoma atractylodis are as the report of plant pesticide.
Summary of the invention
The technical problem that the present invention will solve is the defective that overcomes prior art, and a kind of novel plant insecticide that pollutes little, environmental protection and preparation method thereof is provided.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
One vegetative insecticide, each component and constituent mass percentage are: eucalyptol mother liquor 1-30%, emulsifier 5-20%, surplus are absolute ethyl alcohol; The mass fraction of eucalyptol is 60-90% in the said eucalyptol mother liquor.
Further, the mass fraction of eucalyptol is 5% in the said insecticide.
Further, each component and constituent mass percentage are: the eucalyptol mass fraction is that 80% eucalyptol mother liquor 6.25%, emulsifier 10%, surplus are that absolute ethyl alcohol or eucalyptol mass fraction are that 70% eucalyptol mother liquor 7.14%, emulsifier 10%, surplus are absolute ethyl alcohol.
Further, a vegetative insecticide, said emulsifier is the polyethenoxy ether class nonionic emulsifier.
Further, said emulsifier is an APES.
The preparation method of an above-mentioned vegetative insecticide may further comprise the steps:
(1) preparation of eucalyptol mother liquor:
(a) blue gum and rhizoma atractylodis are cut into segment;
(b) will shear good raw material and join in the extractor, and add clear water again and do not have raw material to get final product, and soak 1-3h, wherein the mass ratio of blue gum and rhizoma atractylodis is 1-5:1;
(c) the logical steam of extractor makes the temperature of extractor remain 50-80 ℃, and constant temperature stirred 3-12 hour; After stopping to stir, stop the steam cooled extractor, when to be extracted jar temperature is reduced to room temperature, pot liquid is passed to oil water separator through filter, obtain thick essential oil;
(d) the thick essential oil that step (c) is obtained passes to destilling tower, collects 70-90 ℃ distillate, and promptly the eucalyptol mass fraction is the eucalyptol mother liquor of 60-90%;
(2) be mixed: the eucalyptol mass fraction that in agitated reactor, adds proportional quantity successively is eucalyptol mother liquor, emulsifier and the absolute ethyl alcohol of 60-90%, stirs 30-120min then, obtains vegetable insecticide.
Further, (c) middle extractor passes through cooling water temperature in the preparation of said step (1) eucalyptol mother liquor.
Further, (c) makes the temperature of extractor remain 60 ℃ for the logical steam of extractor in the preparation of said step (1) eucalyptol mother liquor, and constant temperature stirred 6 hours; After stopping to stir, stop water flowing cooling extractor behind the steam, when to be extracted jar temperature is reduced to room temperature; Pot liquid is passed to oil water separator through filter, obtain thick essential oil.
Further, said emulsifier is the polyethenoxy ether class nonionic emulsifier.
Further, said emulsifier is an APES.
The novel plant insecticide that obtains of the present invention is a soluble liquid.
Eucalyptol (Qleum Eucalypti) is that myrtle blue gum Eucalyptus globulus Labill, canella camphor tree Cinnamomum camphora (L.) Sieb. or above-mentioned two kinds belong to other plant together and obtain volatile oil through steam distillation.These plants are perennial high megaphanerophyte, and South China Tropical, subtropical zone distribute and be tame more, aboundresources.The main component of volatile oil extracted from eucalyptus' leaves or twigs is volatile oil extracted from eucalyptus' leaves or twigs (C10H18O), and content is not less than 70% in oil.According to bibliographical information folium eucalypti decoction and volatile oil extracted from eucalyptus' leaves or twigs desinsection, sterilization functions and anti-corrosive fresh-keeping effect are arranged, stored grain insects are also had fumigating insect killing action.
Rhizoma atractylodis Attactylodes chinensis (Bge.) Koidz. is the composite family perennial plant.Contain essential oil, in the oil main component be atractylol (Atractylol, C15H26O).According to bibliographical information, rhizoma atractylodis have desinsection and controlling plant diseases effect, can kill pest such as mosquito (comprising its larva), stored grain insects, decayed tooth.
The present invention is on the basis of a large amount of lab screenings, confirms with the blue gum proportioning to be primary raw material with Chinese herbal medicines such as rhizoma atractylodis, extracts and is processed into mother liquor, adds auxiliary agents such as emulsifier and absolute ethyl alcohol.Vegetable insecticide of the present invention is to initiate both at home and abroad, and the toxicity of agents useful for same is less, not only environmental protection but also safety when manipulating.
The eucalyptol mass fraction that the present invention prepares is 5% vegetable insecticide control vegetable aphid field control effectiveness test
One, test material and method:
1, experimental field basic condition: the experimental field is located at Da Yang township, Qingyuan County, Baoding, Hebei province, sandy loam, and soil fertility is better, and water waters the field, throughout the year planting vegetable.
2, trial crops and tillage and cultivation: sowing on August 7 calendar year 2001, field planting on August 26, breeds of Chinese cabbage is " rich anti-8 0 ", 50 centimetres of line-spacings, 45 centimetres of spacing in the rows.
3, supply the reagent agent: contain the eucalyptol mass fraction and be 5% novel plant insecticide (hereinafter to be referred as 5% eucalyptol soluble liquid).
4, supply the examination insect: vegetable aphid (hang with black peach aphid Myzus persicae Sulzer and dish to manage oyster Lipaphis ervsimi pscUdooi-assicae Davis be main) moderate generation in the current year.
5, test Treatment Design: 5% eucalyptol soluble liquid preparation consumption 750ml/ha. (1000 times), 5% eucalyptol soluble liquid preparation consumption 1000ml/ ha. (750 times), 5% eucalyptol soluble liquid preparation consumption 1500ml/ha. (500 times) are established in test, and contrasting medicament 2. 5% cream of decamethrin 375ml/ha. (2000 times) and not spraying medicine is blank.Repeat for four times, amount to 20 experimental plots, district's group is arranged at random, 25 square metres of every sub-district areas.
6, dispenser date and application method: calendar year 2001 dispenser on September 15 once, with manual type sprayer (bodyguard WS-16 type), every mu with 50 kilograms of soups (7 50 kilograms/hectare).Soup evenly all is sprayed at each position of Chinese cabbage hand and foot.
7, duration of test meteorological condition: dispenser was fine the same day, did not have rainfall in seven days after the dispenser.
8, experimental field natural enemy situation: the field natural enemy is less, and a small amount of ladybug is arranged.
9, investigation method and statistical analysis:
(1) investigation method: 5 samplings in every sub-district, every 2 Chinese cabbage, every sub-district mark is altogether investigated 10.Investigation radix before the dispenser, l, 3,7 days investigation record aphid numbers alive after the dispenser.
(2) statistical effect: represent control efficiency to proofread and correct the insect population rate of going down, carry out statistical computation according to medicine inspecting institute of the Ministry of Agriculture " pesticide field efficacy medicine test criterion () " prescriptive procedure.
Two, result of the test and evaluation
1, test result analysis: the pilot survey data are seen table 2, and table 1 is seen in result of the test and statistical analysis.Find out that from table 1 5% eucalyptol soluble liquid preparation consumption 1500 ml/ha. and 1000 ml/ha. handle has the better prevention effect to vegetable aphid, can effectively control causing harm of vegetable aphid.Can find out from statistics; The 3rd, 7 days control efficiency of 5% eucalyptol soluble liquid, 1500 ml/ha. is respectively 90.3% and 88. 8%; The 3rd, 7 days control efficiency of 5% eucalyptol soluble liquid, 1000 ml/ha. is respectively 87. 2% and 85. 0%, and control efficiency is all more than 8 5%.5% eucalyptol soluble liquid, 1500 ml/ha. handle the preventive effect of handling the 1st, 3,7 day with contrast medicament 2.5% cream of decamethrin 375ml/ha. does not have significant difference, all is significantly higher than the preventive effect that this medicament 750ml/ha. handles; 5% eucalyptol soluble liquid, 750 ml/ha. handle the 3rd day preventive effect and reach 78. 6%, and preventive effect is lower.5% eucalyptol soluble liquid 1500ml/ha. handles the 1st day, the 7th day preventive effect
Be respectively 86. 8% and 88. 8%, show good quick-acting and lasting effect.
2, to the influence of natural enemy: through field observation, test supplies the reagent agent to handle has lethal effect to natural enemies such as ladybugs.
3, to the influence of crop: through field observation, supply the reagent agent under test dose to crop safety.
Three, conclusion:
5% eucalyptol soluble liquid control Chinese cabbage vegetable aphid has higher preventive effect; Preparation consumption 1000-1500rnl/ha. handles the 7th day preventive effect 85. 0%-88. 8%; Chinese cabbage there is not poisoning; Can apply aborning, exemplary application dosage is advisable with preparation consumption 1000-1500ml/ha..
Table 1 5% eucalyptol soluble liquid control vegetable aphid field trial statistics table
Annotate: preventive effect is carried out variance analysis in the * table after the arcsine conversion, and carries out multiple ratio with the Deng Kenshi duncan's new multiple range method, has same letter person in the same column on 0.05 level, not have significant difference.
Table 2 5% eucalyptol soluble liquid control vegetable aphid field trial survey data
The eucalyptol mass fraction that the present invention prepares is 0.6% vegetable insecticide control vegetable aphid field control effectiveness test
One, test material and method: communicate with the test of pesticide effectiveness of 5% eucalyptol soluble liquid.
Two, conclusion: 0.6% eucalyptol soluble liquid control Chinese cabbage vegetable aphid; Preparation consumption 8830-12500ml/ha. handles the 7th day preventive effect 80.0%-87.5%; Chinese cabbage there is not poisoning; Can apply aborning, exemplary application dosage is advisable with preparation consumption 8830-12500ml/ha..
Table 3 0.6% eucalyptol soluble liquid control vegetable aphid field trial statistics table
Annotate: preventive effect is carried out variance analysis in the * table after the arcsine conversion, and carries out multiple ratio with the Deng Kenshi duncan's new multiple range method, has same letter person in the same column on 0.05 level, not have significant difference.
Table 4 0.6% eucalyptol soluble liquid control vegetable aphid field trial survey data
The eucalyptol mass fraction that the present invention prepares is 4% vegetable insecticide control vegetable aphid field control effectiveness test
One, test material and method: communicate with the test of pesticide effectiveness of 5% eucalyptol soluble liquid.
Two, conclusion: 4% eucalyptol soluble liquid control Chinese cabbage vegetable aphid; Preparation consumption 1250-1875ml/ha. handles the 7th day preventive effect 80.8%-86.5%; Chinese cabbage there is not poisoning; Can apply aborning, exemplary application dosage is advisable with preparation consumption 8830-12500ml/ha..
Table 5 4% eucalyptol soluble liquid control vegetable aphid field trial statistics table
Annotate: preventive effect is carried out variance analysis in the * table after the arcsine conversion, and carries out multiple ratio with the Deng Kenshi duncan's new multiple range method, has same letter person in the same column on 0.05 level, not have significant difference.
Table 6 4% eucalyptol soluble liquid control vegetable aphid field trial survey data
The eucalyptol mass fraction that the present invention prepares is 5.5% vegetable insecticide control vegetable aphid field control effectiveness test
One, test material and method: communicate with the test of pesticide effectiveness of 5% eucalyptol soluble liquid.
Two, conclusion: 5.5% eucalyptol soluble liquid control Chinese cabbage vegetable aphid; Preparation consumption 1250-1875ml/ha. handles the 7th day preventive effect 84.3%-86.4%; Chinese cabbage there is not poisoning; Can apply aborning, exemplary application dosage is advisable with preparation consumption 909-1364ml/ha..
Table 7 5.5% eucalyptol soluble liquid control vegetable aphid field trial statistics table
Annotate: preventive effect is carried out variance analysis in the * table after the arcsine conversion, and carries out multiple ratio with the Deng Kenshi duncan's new multiple range method, has same letter person in the same column on 0.05 level, not have significant difference.
Table 8 5.5% eucalyptol soluble liquid control vegetable aphid field trial survey data
The eucalyptol mass fraction that the present invention prepares is 27% vegetable insecticide control vegetable aphid field control effectiveness test
One, test material and method: communicate with the test of pesticide effectiveness of 5% eucalyptol soluble liquid.
Two, conclusion: 27% eucalyptol soluble liquid control Chinese cabbage vegetable aphid has higher preventive effect; Preparation consumption 185-278 ml/ha. handles the 7th day preventive effect 82.0%-88.5%; Chinese cabbage there is not poisoning; Can apply aborning, exemplary application dosage is advisable with preparation consumption 185-278ml/ha..
Table 9 5% eucalyptol soluble liquid control vegetable aphid field trial statistics table
Annotate: preventive effect is carried out variance analysis in the * table after the arcsine conversion, and carries out multiple ratio with the Deng Kenshi duncan's new multiple range method, has same letter person in the same column on 0.05 level, not have significant difference.
Table 10 27% eucalyptol soluble liquid control vegetable aphid field trial survey data
Each component of the insecticide of the above-mentioned test of pesticide effectiveness and set of dispense are such as table 11
Each component of the insecticide of the above-mentioned test of pesticide effectiveness of table 11 and set of dispense ratio
Embodiment
Below in conjunction with accompanying drawing the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for explanation and explains the present invention, and be not used in qualification the present invention.
Embodiment 1
One vegetative insecticide, each component and constituent mass percentage are: containing the eucalyptol mass fraction and be 60% eucalyptol mother liquor 1%, emulsifier 5%, surplus is absolute ethyl alcohol.
Emulsifier is the polyethenoxy ether class nonionic emulsifier, is specially APES.
The preparation method of an above-mentioned vegetative insecticide may further comprise the steps:
(1) preparation of eucalyptol mother liquor:
(a) the manual work cured leaf of removing blue gum leaf and spray and rhizoma atractylodis leaf spray is done branch, then blue gum leaf and spray and rhizoma atractylodis leaf and spray is cut into segment;
(b) will shear good raw material and join in the extractor, and add clear water again and do not have raw material to get final product, and soak 1h, wherein the mass ratio of blue gum leaf spray and rhizoma atractylodis leaf spray is 1:1;
(c) the logical steam of extractor makes the temperature of extractor remain 50 ℃, and constant temperature stirred 3 hours; After stopping to stir, stop passing through the water quench extractor behind the steam, when to be extracted jar temperature is reduced to room temperature, pot liquid is passed to oil water separator through filter, obtain thick essential oil;
(d) the thick essential oil that step (c) is obtained passes to destilling tower, collects 70 ℃ distillate, i.e. the eucalyptol mother liquor;
(e) utilize the content of the eucalyptol in the gas chromatography determination eucalyptol mother liquor: use the acetone solution sample; With ethyl acetate is internal standard compound; Use fusion capillary column and hydrogen ion detector (FID); Carry out quantitatively according to internal standard method, examination criteria is Q/PGYGN003-2008, records that the eucalyptol mass fraction is about 60% in the eucalyptol mother liquor that step (d) obtains;
(2) be mixed: in agitated reactor, adding 94g absolute ethyl alcohol, 1g successively, to contain the eucalyptol mass fraction be 60% eucalyptol mother liquor and 5g emulsifier, stirs 30min then, obtains vegetable insecticide.
Sampling detects at the bottom of the still, and examination criteria is Q/PGYGN003-2008, and the mass fraction of eucalyptol is 0.6% in the novel plant insecticide for preparing.
The formulation of above-mentioned vegetable insecticide is a soluble liquid.
Embodiment 2
One vegetative insecticide, each component and constituent mass percentage are: containing the eucalyptol mass fraction and be 70% eucalyptol mother liquor 7.14%, emulsifier 10%, surplus is absolute ethyl alcohol.
Emulsifier is the polyethenoxy ether class nonionic emulsifier, is specially APES.
The preparation method of an above-mentioned vegetative insecticide may further comprise the steps:
(1) preparation of eucalyptol mother liquor:
(a) the manual work cured leaf of removing blue gum leaf and spray and rhizoma atractylodis leaf spray is done branch, then blue gum leaf and spray and rhizoma atractylodis leaf and spray is cut into segment;
(b) will shear good raw material and join in the extractor, and add clear water again and do not have raw material to get final product, and soak 2h, wherein the mass ratio of blue gum leaf spray and rhizoma atractylodis leaf spray is 2:1;
(c) the logical steam of extractor makes the temperature of extractor remain 60 ℃, and constant temperature stirs 6h; After stopping to stir, stop passing through the water quench extractor behind the steam, when to be extracted jar temperature is reduced to room temperature, pot liquid is passed to oil water separator through filter, obtain thick essential oil;
(d) the thick essential oil that step (c) is obtained passes to destilling tower, collects 80 ℃ distillate, i.e. the eucalyptol mother liquor;
(e) utilize the content of the eucalyptol in the gas chromatography determination eucalyptol mother liquor: use the acetone solution sample; With ethyl acetate is internal standard compound; Use fusion capillary column and hydrogen ion detector (FID); Carry out quantitatively according to internal standard method, examination criteria is Q/PGYGN003-2008, records that the eucalyptol mass fraction is about 70% in the eucalyptol mother liquor that step (d) obtains;
(2) be mixed: in agitated reactor, adding 82.86g absolute ethyl alcohol, 7.14g successively, to contain the eucalyptol mass fraction be 70% eucalyptol mother liquor and 10g emulsifier, stirs 60min then, obtains vegetable insecticide.
Sampling detects at the bottom of the still, and examination criteria is Q/PGYGN003-2008, and the mass fraction of eucalyptol is 5% in the novel plant insecticide for preparing.
The formulation of above-mentioned vegetable insecticide is a soluble liquid.
Embodiment 3
One vegetative insecticide, each component and constituent mass percentage are: containing the eucalyptol mass fraction and be 90% eucalyptol mother liquor 22.22%, emulsifier 20%, surplus is absolute ethyl alcohol.
Emulsifier is the polyethenoxy ether class nonionic emulsifier, is specially APES.
The preparation method of an above-mentioned vegetative insecticide may further comprise the steps:
(1) preparation of eucalyptol mother liquor:
(a) the manual work cured leaf of removing blue gum leaf and spray and rhizoma atractylodis leaf spray is done branch, then blue gum leaf and spray and rhizoma atractylodis leaf and spray is cut into segment;
(b) will shear good raw material and join in the extractor, and add clear water again and do not have raw material to get final product, and soak 3h, wherein the mass ratio of blue gum leaf spray and rhizoma atractylodis leaf spray is 5:1;
(c) the logical steam of extractor makes the temperature of extractor remain 80 ℃, and constant temperature stirs 12h; After stopping to stir, stop passing through the water quench extractor behind the steam, when to be extracted jar temperature is reduced to room temperature, pot liquid is passed to oil water separator through filter, obtain thick essential oil;
(d) the thick essential oil that step (c) is obtained passes to destilling tower, collects 80 ℃ distillate, i.e. the eucalyptol mother liquor;
(e) utilize the content of the eucalyptol in the gas chromatography determination eucalyptol mother liquor: use the acetone solution sample; With ethyl acetate is internal standard compound; Use fusion capillary column and hydrogen ion detector (FID); Carry out quantitatively according to internal standard method, examination criteria is Q/PGYGN003-2008, records that the eucalyptol mass fraction is about 90% in the eucalyptol mother liquor that step (d) obtains;
(2) be mixed: in agitated reactor, adding 57.78g absolute ethyl alcohol, 22.22g successively, to contain the eucalyptol mass fraction be 90% eucalyptol mother liquor and 20g emulsifier, stirs 120min then, obtains vegetable insecticide.
Sampling detects at the bottom of the still, and examination criteria is Q/PGYGN003-2008, and the mass fraction of eucalyptol is 20% in the novel plant insecticide for preparing.
The formulation of above-mentioned vegetable insecticide is a soluble liquid.
Embodiment 4
One vegetative insecticide, each component and constituent mass percentage are: containing the eucalyptol mass fraction and be 90% eucalyptol mother liquor 30%, emulsifier 20%, surplus is absolute ethyl alcohol.
Emulsifier is the polyethenoxy ether class nonionic emulsifier, is specially APES.
The preparation method of an above-mentioned vegetative insecticide may further comprise the steps:
(1) preparation of eucalyptol mother liquor:
(a) the manual work cured leaf of removing blue gum leaf and spray and rhizoma atractylodis leaf spray is done branch, then blue gum leaf and spray and rhizoma atractylodis leaf and spray is cut into segment;
(b) will shear good raw material and join in the extractor, and add clear water again and do not have raw material to get final product, and soak 3h, wherein the mass ratio of blue gum leaf spray and rhizoma atractylodis leaf spray is 5:1;
(c) the logical steam of extractor makes the temperature of extractor remain 80 ℃, and constant temperature stirs 12h; After stopping to stir, stop cooling off extractor through the nature cooling behind the steam, when to be extracted jar temperature is reduced to room temperature, pot liquid is passed to oil water separator through filter, obtain thick essential oil;
(d) the thick essential oil that step (c) is obtained passes to destilling tower, collects 80 ℃ distillate, i.e. the eucalyptol mother liquor;
(e) utilize the content of the eucalyptol in the gas chromatography determination eucalyptol mother liquor: use the acetone solution sample; With ethyl acetate is internal standard compound; Use fusion capillary column and hydrogen ion detector (FID); Carry out quantitatively according to internal standard method, examination criteria is Q/PGYGN003-2008, records that the eucalyptol mass fraction is about 90% in the eucalyptol mother liquor that step (d) obtains;
(2) be mixed: in agitated reactor, adding 100g absolute ethyl alcohol, 60g successively, to contain the eucalyptol mass fraction be 90% eucalyptol mother liquor and 40g emulsifier, stirs 120min then, obtains vegetable insecticide.
Sampling detects at the bottom of the still, and examination criteria is Q/PGYGN003-2008, and the mass fraction of eucalyptol is 27% in the novel plant insecticide for preparing.
The formulation of above-mentioned vegetable insecticide is a soluble liquid.
Embodiment 5
One vegetative insecticide, each component and constituent mass percentage are: containing the eucalyptol mass fraction and be 60% eucalyptol mother liquor 9.1%, emulsifier 5%, surplus is absolute ethyl alcohol.
Emulsifier is the polyethenoxy ether class nonionic emulsifier, is specially APES.
The preparation method of an above-mentioned vegetative insecticide may further comprise the steps:
(1) preparation of eucalyptol mother liquor:
(a) the manual work cured leaf of removing blue gum leaf and spray and rhizoma atractylodis leaf spray is done branch, then blue gum leaf and spray and rhizoma atractylodis leaf and spray is cut into segment;
(b) will shear good raw material and join in the extractor, and add clear water again and do not have raw material to get final product, and soak 3h, wherein the mass ratio of blue gum leaf spray and rhizoma atractylodis leaf spray is 1:1;
(c) the logical steam of extractor makes the temperature of extractor remain 80 ℃, and constant temperature stirs 12h; After stopping to stir, stop cooling off extractor through the nature cooling behind the steam, when to be extracted jar temperature is reduced to room temperature, pot liquid is passed to oil water separator through filter, obtain thick essential oil;
(d) the thick essential oil that step (c) is obtained passes to destilling tower, collects 80 ℃ distillate, i.e. the eucalyptol mother liquor;
(e) utilize the content of the eucalyptol in the gas chromatography determination eucalyptol mother liquor: use the acetone solution sample; With ethyl acetate is internal standard compound; Use fusion capillary column and hydrogen ion detector (FID); Carry out quantitatively according to internal standard method, examination criteria is Q/PGYGN003-2008, records that the eucalyptol mass fraction is about 60% in the eucalyptol mother liquor that step (d) obtains;
(2) be mixed: in agitated reactor, adding 171.8g absolute ethyl alcohol, 18.2g successively, to contain the eucalyptol mass fraction be 60% eucalyptol mother liquor and 10g emulsifier, stirs 120min then, obtains vegetable insecticide.
Sampling detects at the bottom of the still, and examination criteria is Q/PGYGN003-2008, and the mass fraction of eucalyptol is 5.5% in the novel plant insecticide for preparing.
The formulation of above-mentioned vegetable insecticide is a soluble liquid.
Embodiment 6
One vegetative insecticide, each component and constituent mass percentage are: containing the eucalyptol mass fraction and be 90% eucalyptol mother liquor 4.5%, emulsifier 10%, surplus is absolute ethyl alcohol.
Emulsifier is the polyethenoxy ether class nonionic emulsifier, is specially APES.
The preparation method of an above-mentioned vegetative insecticide may further comprise the steps:
(1) preparation of eucalyptol mother liquor:
(a) the manual work cured leaf of removing blue gum leaf and spray and rhizoma atractylodis leaf spray is done branch, then blue gum leaf and spray and rhizoma atractylodis leaf and spray is cut into segment;
(b) will shear good raw material and join in the extractor, and add clear water again and do not have raw material to get final product, and soak 3h, wherein the mass ratio of blue gum leaf spray and rhizoma atractylodis leaf spray is 5:1;
(c) the logical steam of extractor makes the temperature of extractor remain 80 ℃, and constant temperature stirs 12h; After stopping to stir, stop cooling off extractor through the nature cooling behind the steam, when to be extracted jar temperature is reduced to room temperature, pot liquid is passed to oil water separator through filter, obtain thick essential oil;
(d) the thick essential oil that step (c) is obtained passes to destilling tower, collects 80 ℃ distillate, i.e. the eucalyptol mother liquor;
(e) utilize the content of the eucalyptol in the gas chromatography determination eucalyptol mother liquor: use the acetone solution sample; With ethyl acetate is internal standard compound; Use fusion capillary column and hydrogen ion detector (FID); Carry out quantitatively according to internal standard method, examination criteria is Q/PGYGN003-2008, records that the eucalyptol mass fraction is about 90% in the eucalyptol mother liquor that step (d) obtains;
(2) be mixed: in agitated reactor, adding 256.5g absolute ethyl alcohol, 13.5g successively, to contain the eucalyptol mass fraction be 90% eucalyptol mother liquor and 30g emulsifier, stirs 120min then, obtains vegetable insecticide.
Sampling detects at the bottom of the still, and examination criteria is Q/PGYGN003-2008, and the mass fraction of eucalyptol is 4% in the novel plant insecticide for preparing.
The formulation of above-mentioned vegetable insecticide is a soluble liquid.
What should explain at last is: the above is merely the preferred embodiments of the present invention; Be not limited to the present invention; Although the present invention has been carried out detailed explanation with reference to previous embodiment; For a person skilled in the art, it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a vegetative insecticide is characterized in that, each component and constituent mass percentage are: eucalyptol mother liquor 1-30%, emulsifier 5-20%, surplus are absolute ethyl alcohol; The mass fraction of eucalyptol is 60-90% in the said eucalyptol mother liquor.
2. a vegetative insecticide according to claim 1 is characterized in that: the mass fraction of eucalyptol is 5% in the said insecticide.
3. a vegetative insecticide according to claim 2; It is characterized in that each component and constituent mass percentage are: the eucalyptol mass fraction is that 80% eucalyptol mother liquor 6.25%, emulsifier 10%, surplus are that absolute ethyl alcohol or eucalyptol mass fraction are that 70% eucalyptol mother liquor 7.14%, emulsifier 10%, surplus are absolute ethyl alcohol.
4. according to each described vegetative insecticide of claim 1-3, it is characterized in that: said emulsifier is the polyethenoxy ether class nonionic emulsifier.
5. a vegetative insecticide according to claim 4 is characterized in that: said emulsifier is an APES.
6. according to the preparation method of each described vegetative insecticide of claim 1-3, it is characterized in that, may further comprise the steps:
(1) preparation of eucalyptol mother liquor:
(a) blue gum and rhizoma atractylodis are cut into segment;
(b) will shear good raw material and join in the extractor, and add clear water again and do not have raw material to get final product, and soak 1-3h, wherein the mass ratio of blue gum and rhizoma atractylodis is 1-5:1;
(c) the logical steam of extractor makes the temperature of extractor remain 50-80 ℃, and constant temperature stirred 3-12 hour; After stopping to stir, stop the steam cooled extractor, when to be extracted jar temperature is reduced to room temperature, pot liquid is passed to oil water separator through filter, obtain thick essential oil;
(d) the thick essential oil that step (c) is obtained passes to destilling tower, collects 70-90 ℃ distillate, and promptly the eucalyptol mass fraction is the eucalyptol mother liquor of 60-90%;
(2) be mixed: the eucalyptol mass fraction that in agitated reactor, adds proportional quantity successively is eucalyptol mother liquor, emulsifier and the absolute ethyl alcohol of 60-90%, stirs 30-120min then, obtains vegetable insecticide.
7. the preparation method of a vegetative insecticide according to claim 6 is characterized in that: (c) middle extractor passes through cooling water temperature in the preparation of said step (1) eucalyptol mother liquor.
8. the preparation method of a vegetative insecticide according to claim 7 is characterized in that: (c) makes the temperature of extractor remain 60 ℃ for the logical steam of extractor in the preparation of said step (1) eucalyptol mother liquor, and constant temperature stirred 6 hours; After stopping to stir, stop water flowing cooling extractor behind the steam, when to be extracted jar temperature is reduced to room temperature; Pot liquid is passed to oil water separator through filter, obtain thick essential oil.
9. the preparation method of a vegetative insecticide according to claim 6 is characterized in that: said emulsifier is the polyethenoxy ether class nonionic emulsifier.
10. the preparation method of a vegetative insecticide according to claim 9 is characterized in that: said emulsifier is an APES.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104920492A (en) * | 2015-06-12 | 2015-09-23 | 福建省德盛生物工程有限责任公司 | Low-volume spray containing eucalyptol |
| CN107156207A (en) * | 2017-06-01 | 2017-09-15 | 磐安县派普特生物科技有限公司 | A kind of vegetable source natural insecticide and preparation method thereof |
| CN112042682A (en) * | 2020-09-07 | 2020-12-08 | 衡东林馨农林科技开发有限责任公司 | Preparation method of plant insecticide for fruit tree planting |
| WO2022199653A1 (en) * | 2021-03-26 | 2022-09-29 | 江南大学 | Method for preparing eucalyptol emulsion and application thereof in biopesticide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086961A (en) * | 1992-11-19 | 1994-05-25 | 西北农业大学 | Celastrus angulatus emulsified oil as plant's pesticide and manufacture method thereof |
| CN1826903A (en) * | 2006-04-13 | 2006-09-06 | 华南农业大学 | Insect and mite killer with vegetable oil as base |
| CN101427694A (en) * | 2007-11-08 | 2009-05-13 | 冷雪飞 | Natural green biological organic agricultural chemical composition and uses thereof |
| CN102038011A (en) * | 2009-10-20 | 2011-05-04 | 王海军 | Spray for killing insects and flies |
-
2011
- 2011-06-23 CN CN 201110171300 patent/CN102626116B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086961A (en) * | 1992-11-19 | 1994-05-25 | 西北农业大学 | Celastrus angulatus emulsified oil as plant's pesticide and manufacture method thereof |
| CN1826903A (en) * | 2006-04-13 | 2006-09-06 | 华南农业大学 | Insect and mite killer with vegetable oil as base |
| CN101427694A (en) * | 2007-11-08 | 2009-05-13 | 冷雪飞 | Natural green biological organic agricultural chemical composition and uses thereof |
| CN102038011A (en) * | 2009-10-20 | 2011-05-04 | 王海军 | Spray for killing insects and flies |
Non-Patent Citations (3)
| Title |
|---|
| 《药用植物研究与中药现代化--第四届全国药用植物学与植物药学术研讨会论文集》 20041231 李艾莲等 植物源农药"5%桉油精可溶性液剂"药效试验 第418页 1-10 , * |
| 李占富等: "5%桉油精防治杨树食叶害虫试验", 《中国森林病虫》 * |
| 李艾莲等: "植物源农药"5%桉油精可溶性液剂"药效试验", 《药用植物研究与中药现代化——第四届全国药用植物学与植物药学术研讨会论文集》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104920492A (en) * | 2015-06-12 | 2015-09-23 | 福建省德盛生物工程有限责任公司 | Low-volume spray containing eucalyptol |
| CN107156207A (en) * | 2017-06-01 | 2017-09-15 | 磐安县派普特生物科技有限公司 | A kind of vegetable source natural insecticide and preparation method thereof |
| CN112042682A (en) * | 2020-09-07 | 2020-12-08 | 衡东林馨农林科技开发有限责任公司 | Preparation method of plant insecticide for fruit tree planting |
| WO2022199653A1 (en) * | 2021-03-26 | 2022-09-29 | 江南大学 | Method for preparing eucalyptol emulsion and application thereof in biopesticide |
| US11980186B2 (en) * | 2021-03-26 | 2024-05-14 | Jiangnan University | Preparation method of eucalyptol emulsion and application thereof in biopesticides |
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| CN102626116B (en) | 2013-09-04 |
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